Treatment of mined sulfur



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R. F. .BACON lAND H. .,s. DAVIS. TREATMENT v(IMF IVI-INED SfU'L-FUR.

` APPLICATION FILED "0lCz'l'..\6| AI'9I9. 1,374,898, Patented Apr. 19, 1921.

UNITED STA-TES PATENT ',oFFIcE.

,RAYMOND r. BAcoN AND HAROLD s. DAvIs, or PITTSBURGH, PENNSYLVANIA ASSIGNORS TO TEXAS GULF SULPHUR COMPANY, 0F BAY CITY, TEXAS, y.A

CORPORATION OF TEXAS.

TREATMENT 0F MINED SULFUR.

i La7-.nega` Specication of Letters Patent. Patented Api'.y I9, 1921.

Application led October 6, 1.919. Serial No. 328,935. l n

'To all whom t many conce/m i Be it known that we, RAYMOND'F. BACON,I

a citizen of the United States, and HAROLD S. DAvIsa citizen of the Dominion of` Canada, both residing in Pittsburgh, Allegheny county, State of Pennsylvania, have invented certain new and useful Improvements in the Treatment of Mined Sulfur, `(Case B;) and we do hereby declare the following'tolbe a full, clear, and exact description of the invention, such'as will enable others skilled` in the art to which `it appertains to make and use the same.

In an application filed of even date herewith, we have described a method for improving the free burning properties of mined sulfur, by maintaining a molten body of the sulfur at a temperature' sulicient to carbonize the oil contained therein.

The present yapplication contemplates not only the carbonizing-of the oil by the method referred to, but also the elimination of the carbon from the sulfur, so that the final product shall be of a grade comparable Ato an'duseful for purposes for which krefined sulfur is now employed in the arts.

In carrying out the invention, the mined sulfur, as fully described in our application hereinbefore referred to, is delivered into a receptacle (preferably in a molten condition, and direct from the mine or from some other source of molten sulfur supply) and is heatedtherein, for a sufficient length of time, to a temperature sufficient to carbonize the oil. The receptacle may conveniently be contained within a furnace structure, provided with suitable fuel burners or other `,heating elements, and having preferably y' such adjuncts as heat-storing checker-work 40.

tol maintain and distribute the heat generated by the combustion of the fuel. So also,

as will be understood, the furnace structure may be provided with a suitablev exit flue for the produc-ts of combustion, and the receptacle may be provided with a suitable take-ofi' pipe for hydrogen suld and whatever vapors may be disengaged in the heating operation. F urthermore,the uniformity of the heating operation may be assured by providing the receptacle with a suitable agitating device. y

We have found that the carbonizing of the oil may be carried on at temperatures Within a considerable range, providedthat effectually removed in the subsequent stages of the operation, leaving a final product which cools to a brilliant lemon color, as will hereinafter more fully appear.

We have discovered that if, atthe termination of the oil-carbonizing operation, op-I o portunity is given the molten mass, under proper conditions, to cool to a lower'temperature but without ,solidifyingg and ifI this lower` temperature is maintained for a sufficient lengthof time, the carbon will segregate out from the mass in distributed groups of aggregated particles, capable of separation by settling, filtration, or the like. The preferred range of thisloiver temperature is from 120o C. to 140 C., or thereabouts` and the molten mass is preferably transferred to another receptacle entirely Noutsideof the furnace structure, and of considerably larger dimensions, so that the cooling operatlon may not be unduly delayed. In this second receptacle, the temperature of the mass is brought as quickly as possible to the range of'120.C. to 140o C., or thereabouts, re-

ferred to, and it is maintained at that temperature for a period of about two days. It is found that during this interval, the carbon, as above noted, segregates out from the mass in distributed groups of aggregated particles, and in such manner that it may then be separated either by settling or filtration. The addition of fullers earth, or like discharge pipe as shown. The receptacle B is provided with a cover b, a'valved inlet pipe c for the admission ofthe molten sulfur and an exit flue d for the escape ofhydrogen sulfid or any other vapors given ofi'l diurlng the operation. provided with any suitable exit fiue f for the roducts of combustion and may be heated by a fuel injector burner, indicated by e, or the like. h 'indicates suitable heat-storing brick-work serving as a heat storer and distributer; and z' indicates a rotary paddle or the like whose shaft fm is driven from any suitable source of power as, for instance, by means of the band wheel and belt shown.

fur, and the temperature employed.

As hereinbefore indicated, if the temperature of the sulfur is raised to a range of from 400 to430 C. about four hours will usually be required to complete the desired carbonization of the oil. At lower temperatures, a correspondingly longer period of time will be required, as will be evident and as may be determined by test samples taken. A thermometer t is intended to afford an lindication of the prevailing temperature,

for the information and guidance of the operator.

At the termination of the carbonizing operation the molten sulfur containin the carbon is transferred to the vessel provided with a heating jacket D for the circulation of steam or other heating Huid adapted to maintain the temperature of the mass at from 120 to 140 C'. or thereabout. A thermometer ,7c indicates the temperature.

In the vessel C, the material is main-44 tained molten, preferably at the temperature range referred to, for a sufficient period to permit the small particles of carbon to aggregate into larger particles, which usually requires a period, of aboutl two days or more. Thereupon the separation of the sulfurand carbon can be effected by settling (aided if desired by the addition of fullers earth, or the like), ,but more speedily by sand filtration. Thus, the mass, while still in the niolten condition may be transferred through the valved pipe n to the vessel D containing' a body of filtering sand p, through which the molten sulfur will pass, freely taking its exit through the pipe s and leaving the separated particles vof car- The furnace A .isA

bon on the top of the filter bed. The sulfur thus obtained is free from oil and also from carbon,'and'is thus obtainable inthe form of a product of a bright lemon color and of a quality at least equal to Athat of refined sulfur as found on the market at the present time. 4

It will be noted that we haveshown said filter as provided with a steam jacket D which may,'in some instances, be usefully employed for the purpose of increasing the rapidity of flow o'f the sulfur through-the filter and for preventing clogging'thereof. So also, it may be desirable, as indicated in the drawing, to provide the conduit a with a power-driven endless screw, or the like, for hastening the flow of sulfur through said conduit if it should become sluggish. Above the screw, however, the conduit a will be provided with a cut-off valve as shown.

What we claim is:

1.' The method of refining mined sulfurl containing `oil, which comprises carbonizing the oil by maintaining 'a molten body of the sulfur containing it at an oil-carbonizing temperature until the desired carbonization' cient length of time to permit the segregatingout of the carbon; substantially as described. n

2. The method of refining mined sulfur containing oil, which comprises carbonizing the oil by maintaining a molten body of the sulfur containing it at a temperature varying from about 400 C. to 430o C. until the desired carbonization has been effected, and then holdingI the temperature of the body of sulfur above its melting point for a sufficient length of time to permit the segregating out of the carbon; substantially as described.

3. The method of refining mined sulfur containing oil, which comprises carbonizing the oil by maintaining a molten body of the sulfur containing it at a temperature ranging from about 400 C. to 430 C. until the desired carbonization hasbeen effected, then'holdingthe temperature of the body of sulfur at a range of about 120 C. to 140 C. for a suicient length of-time topermit the particles of carbon to collect in small aggregations throughout the mass and separating the carbon and sulfur; substantially as described.

4. The method of refining mined sulfurl -holding the temperature of the body of sulfur at a rang of about 120 O. t0 140 C. for a suiiicient length of time to permit the particles of carbon to collect in small aggregations throughout the mass, adding fullers earth to hasten such aggregation and separating the carbon and sulfur; Substantially as described.

5. The method of refining mined sulfur containing oil, which comprises carbonizing the oil by maintaining a molten body of the sulfur containing it at an oil-carbonizing temperature until the desired carbonization hasbeen effected, then cooling the body of sulfur to a temperature above the melting point of sulfur and holding the body of sulfur at this lower temperature for a sufficient length of time to permit the segregating` out of the carbon, and passing the body of sulfur while still molten through a filter which is impervious to the segregated carbon; substantially as described. i

6. The method of reining` mined sulfur .containing oil, which comprises carbonizing the oil by maintaining a molten bodyof the sulfur containing it at an oil-carbonizing temperature until the desired carbonization has been effected, then lowering the temperature of the body of sulfur to a point above the melting point of sulfur and maintaining the body of sulfur at this lower temperature for a relatively much longer period than at said oil carbonizing temperature and thereby causing the segregating out of the carbon; substantially as described.

In testimony whereof We aHX our signatures.

RAYMOND F. BACON. HAROLD S, DAVIS. 

